一种内嵌三嗪环酰胺极性基团新型固定相的制备及其在碱性化合物分离中的应用

以γ-氨丙基三乙氧基硅烷为偶联剂,三聚氯氰为反应物,采用固液表面连续反应法,依次与乙二胺、十二酰氯进行亲核取代反应,制备了一种嵌入三嗪环酰胺极性基团的新型反相色谱固定相,并采用元素分析法进行了表征。用制备的固定相装填色谱柱,以商品化C18色谱柱作为参考,对比考察了碱性化合物的分离情况。结果表明,极性三嗪环酰胺基团被成功地键合到硅胶表面,连续制备3次所得固定相的C、N、H含量的最大相对偏差均小于5%,说明制备工艺重现性良好;用制备的固定相装填的色谱柱分离5种苯胺类、4种吡啶类碱性化合物的选择性好,峰形对称。该结果为进一步推进该新型固定相的商品化提供了参考数据。

Preparation of a new stationary phase with s-triazine and amide embedded and its application in separation of basic compounds

A new kind of silica-bonded reserved stationary phase with s-triazine and amide polar groups embedded for HPLC was obtained by step-wise reactions of silica gel with s-triazine, γ-aminopropyltriethoxysilane, ethanediamine and dodecanoyl chloride. The new stationary phase was characterized by elemental analysis. After that, a column packed with the new stationary phase was used to separate basic compounds. A commercial C18 column was also tested under the same chromatographic conditions for comparison. The results indicated that the ligand was successfully bonded to the surface of the silica and the maximum relative deviations of element contents were within 5% for carbon, nitrogen and hydrogen by three times. Furthermore, in the separation of five basic anilines and four basic pyridines, the excellent selectivity and symmetrical peak shapes provided a reference for advancing the commercialization of the new stationary phase.